Sealing plaster and preparation method thereof

Abstract

The invention discloses a sealant and a preparation method thereof, and the sealant comprises the following ingredients in parts by weight: 80-180 parts of base resin containing an isoprene chain segment or an acrylonitrile group, 20-80 parts of a polyolefin elastomer, 10-30 parts of high density polyethylene, 20-60 parts of solid tackifying resin, and 100-150 parts of liquid tackifying resin. The sealing cement gum provided by the invention has good sealing property and adhesion, and also has excellent weather resistance and high and low temperature resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of materials, and in particular to a sealing putty and a preparation method thereof. Background Art

[0002] At present, sealing putty is generally used for moisture-proof sealing of medium and low voltage cables, and sealing of cable ends and joints. Its application scenarios require the product to have good viscosity and be able to bond metal, plastic, and rubber. The sealing putty on the market is mainly used in room temperature environments. As the use temperature gradually decreases, the colloid of the putty gradually hardens, and the adhesion gradually decreases, resulting in the gradual failure of the viscosity. When the temperature is too high, the putty will soften and flow, resulting in failure of the seal. The huge temperature difference between the north and the south is a problem faced by most long-span vehicles. Therefore, in order to meet the sealing protection needs in high and low temperature environments, a putty is needed that can not only remain deformed and flow at high temperatures, but also maintain adhesion in low temperature environments. Summary of the Invention

[0003] In view of the above-mentioned deficiencies in the prior art, the present invention proposes a sealing putty and a preparation method thereof, aiming to solve the problem that the current sealing putty has poor weather resistance and fails at high and low temperatures.

[0004] To achieve the above object, the present invention provides a sealing putty and a preparation method thereof.

[0005] A sealing putty, characterized in that the ingredients of the sealing putty, measured in parts by weight, include: 80-180 parts of a base resin containing an isoprene segment or an acrylonitrile group, 20-80 parts of a polyolefin elastomer, 10-30 parts of a high-density polyethylene, 20-60 parts of a solid tackifying resin, and 100-150 parts of a liquid tackifying resin.

[0006] Optionally, the sealing putty includes 20-60 parts of plasticizer, 160-240 parts of filler and 7-15 parts of additive.

[0007] Optionally, the base resin containing isoprene segments or acrylonitrile groups includes 60-120 parts of butyl rubber and 20-60 parts of nitrile rubber.

[0008] Optionally, the solid tackifying resin is at least one of hydrogenated C5 petroleum resin, hydrogenated C9 petroleum resin, rosin resin, hydrogenated rosin resin, water-white rosin resin, rosin pentaerythritol ester, terpene resin, hydrogenated terpene resin, terpene phenol resin and phenolic resin.

[0009] Optionally, the liquid tackifying resin is polyisobutylene with a molecular weight of 1000-3000.

[0010] Optionally, the plasticizer is at least one of white oil and cyclohexane oil.

[0011] Optionally, the filler is at least one of kaolin, calcium carbonate, white carbon black and clay.

[0012] Optionally, the auxiliary agent includes at least one of stearic acid, zinc stearate, an antioxidant and a silane coupling agent.

[0013] In order to achieve the above object, the present invention also provides a method for preparing sealing putty, comprising the following steps: The base resin containing isoprene segments or acrylonitrile groups, polyolefin elastomer, and high-density polyethylene in the above-mentioned parts by weight are mixed in an internal mixer, the temperature is raised to 110-130° C., and the mixing time is 40-60 minutes to form a base rubber; solid tackifying resin, liquid tackifying resin, filler and additives are added to the base rubber, and the mixture is kneaded and mixed at 100-120° C. for 30-50 minutes; the mixed rubber material is put into an extruder and extruded and formed at 80-100° C. to obtain the sealing putty.

[0014] Optionally, the rotation speed of the internal mixer is 30-50 rpm, and the rotation speed of the kneader is 20-40 rpm.

[0015] The beneficial effects of the present invention are as follows: the sealing putty of the present invention contains a base resin of isoprene segments or acrylonitrile groups, a polyolefin elastomer and high-density polyethylene as main components, and materials such as solid tackifying resin and liquid tackifying resin are added. The long side chain structure of the polyolefin elastomer significantly reduces the regularity of the molecular chain. In a low-temperature environment, the molecular chain of the polyolefin elastomer still maintains high elasticity, which can prevent the putty from hardening. The polyolefin elastomer and the liquid tackifying resin have excellent compatibility. At low temperatures, the liquid tackifying resin migrates from the inside of the colloid formed by the polyolefin elastomer and the liquid tackifying resin to the interface to form a flexible transition layer, thereby enhancing the wettability to substrates such as metals and plastics and improving the low-temperature bonding strength of the putty. The solid tackifying resin undergoes a condensation reaction with the isoprene segments or acrylonitrile groups in the base resin to form a three-dimensional cross-linked network. The cross-linked structure inhibits molecular chain slippage at high temperatures (130°C). At the same time, the high-density polyethylene can enhance the heat resistance of the solid tackifying resin and the base resin in a high-temperature environment to prevent the putty from softening and flowing. The liquid tackifying resin is a low-polarity liquid tackifying resin that is evenly dispersed within the colloid during the mixing process. When the temperature changes, its molecular chains migrate to the bonding interface, filling the micropores on the surface of the substrate, forming a physical anchoring effect, and improving the high-temperature bonding strength of the mortar. The mortar of the present invention has a high bonding strength at high and low temperatures (-40°C ~ 130°C). In addition, the plasticizing effect of the liquid tackifying resin reduces the overall modulus of the mortar, while the cross-linked network of the solid tackifying resin provides rigid support, which can ensure the deformation recovery ability of the mortar of the present invention within high and low temperatures (-40°C ~ 130°C), so that the sealing mortar provided by the present invention not only has good sealing and adhesion properties, but also has excellent weather resistance and high and low temperature resistance. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It should be understood that the following embodiments are only used to explain the present invention and are not used to limit the present invention.

[0017] Unless defined otherwise, all technical and scientific terms used herein have the common meaning in the art to which the claimed subject matter belongs.

[0018] To facilitate understanding of this embodiment, the following explains the symbols, instruments and terms: Polyolefin Elastomer: Polyolefin Elastomer, POE, is a thermoplastic elastomer achieved by in-situ polymerization of ethylene and α-olefin using a metallocene catalyst. The crystalline region of the polyethylene chain (resin phase) acts as a physical crosslinking point and has typical plastic properties. After adding a certain amount of α-olefin (1-butene, 1-hexene, 1-octene, etc.), the crystalline region of the polyethylene chain is weakened, forming an amorphous region (rubber phase) exhibiting rubber elasticity, giving the product the properties of an elastomer, excellent physical and mechanical properties and a wide range of processing applications.

[0019] High-density polyethylene (HDPE) is a plastic material with extremely high density and strength. It is a thermoplastic resin produced from ethylene monomer through a low-pressure polymerization process. Its molecular structure is primarily linear with minimal branching, resulting in high density, high crystallinity, and strong rigidity. It possesses excellent mechanical strength, rigidity, and chemical resistance. Its hardness, tensile strength, and creep properties surpass those of other plastic materials. It also exhibits good wear resistance, electrical insulation, toughness, and cold resistance.

[0020] At present, sealing putty is generally used for moisture-proof sealing of medium and low voltage cables, and sealing of cable ends and joints. Its application scenarios require the product to have good viscosity and be able to bond metal, plastic, and rubber. The sealing putty on the market is mainly used in room temperature environments. As the use temperature gradually decreases, the colloid of the putty gradually hardens, and the adhesion gradually decreases, resulting in the gradual failure of the viscosity. When the temperature is too high, the putty will soften and flow, resulting in failure of the seal. The huge temperature difference between the north and the south is a problem faced by most long-span vehicles. Therefore, in order to meet the sealing protection needs in high and low temperature environments, a putty is needed that can not only remain deformed and flow at high temperatures, but also maintain adhesion in low temperature environments.

[0021] To solve the above problems, the present invention proposes a sealing putty, comprising: 80-180 parts of a base resin containing isoprene segments or acrylonitrile groups, 20-80 parts of POE, 10-30 parts of HDPE, 20-60 parts of a solid tackifying resin, and 100-150 parts of a liquid tackifying resin.

[0022] The sealing putty of the present invention contains a base resin containing isoprene segments or acrylonitrile groups, a polyolefin elastomer and high-density polyethylene as main components, and is added with materials such as a solid tackifying resin and a liquid tackifying resin. The long side chain structure of the polyolefin elastomer significantly reduces the regularity of the molecular chain. In a low-temperature environment, the molecular chain of the polyolefin elastomer still maintains high elasticity, which can prevent the putty from hardening. The polyolefin elastomer and the liquid tackifying resin have excellent compatibility. At low temperatures, the liquid tackifying resin migrates from the interior of the colloid formed by the polyolefin elastomer and the liquid tackifying resin to the interface, forming a flexible transition layer, thereby enhancing the wettability to substrates such as metals and plastics and improving the low-temperature bonding strength of the putty. The solid tackifying resin undergoes a condensation reaction with the isoprene segments or acrylonitrile groups in the base resin to form a three-dimensional cross-linked network. The cross-linked structure inhibits molecular chain slippage at high temperatures (130°C). At the same time, the high-density polyethylene can enhance the heat resistance of the solid tackifying resin and the base resin in a high-temperature environment, thereby preventing the putty from softening and flowing. The liquid tackifying resin is a low-polarity liquid tackifying resin that is evenly dispersed within the colloid during the mixing process. When the temperature changes, its molecular chains migrate to the bonding interface, filling the micropores on the surface of the substrate, forming a physical anchoring effect, and improving the high-temperature bonding strength of the mortar. The mortar of the present invention has a high bonding strength at high and low temperatures (-40°C ~ 130°C). In addition, the plasticizing effect of the liquid tackifying resin reduces the overall modulus of the mortar, while the cross-linked network of the solid tackifying resin provides rigid support, which can ensure the deformation recovery ability of the mortar of the present invention within high and low temperatures (-40°C ~ 130°C), so that the sealing mortar provided by the present invention not only has good sealing and adhesion properties, but also has excellent weather resistance and high and low temperature resistance.

[0023] Furthermore, the sealing putty also includes 20-60 parts of plasticizer, 160-240 parts of filler and 7-15 parts of auxiliary agent.

[0024] Plasticizers can significantly improve the physical properties of rubber products, such as strength, wear resistance and weather resistance, improve the elasticity and toughness of rubber products, and extend the service life of the products. Adding a certain amount of fillers and additives can improve the mechanical properties of each component material and improve the overall performance of the sealing putty.

[0025] In some embodiments, the sealing putty also includes 20-60 parts of plasticizer, 160-240 parts of filler and 5-15 parts of additive. In the above-mentioned "20-60 parts of plasticizer", the value includes the minimum and maximum values of the range, and each value between the minimum and maximum values. Specific examples include but are not limited to the point values in the embodiment and the following point values: 20, 30, 40, 50, 60; in the above-mentioned "160-240 parts of filler", the value includes the minimum and maximum values of the range, and each value between the minimum and maximum values. Specific examples include but are not limited to the point values in the embodiment and the following point values: 160, 170, 180, 190, 200, 210, 220, 230, 240; in the above-mentioned "5-15 parts of additive", the value includes the minimum and maximum values of the range, and each value between the minimum and maximum values. Specific examples include but are not limited to the point values in the embodiment and the following point values: 5, 7, 9, 11, 13, 15.

[0026] Furthermore, the base resin containing isoprene segments or acrylonitrile groups includes 60-120 parts of butyl rubber and 20-60 parts of nitrile rubber.

[0027] The mixture of butyl rubber and nitrile rubber in a base resin containing isoprene segments or acrylonitrile groups can form a "complementary" composite material. The high air tightness of butyl rubber combined with the oil resistance and solvent resistance of nitrile rubber can achieve gas isolation and contact with oils at the same time. The ozone resistance and aging resistance of butyl rubber make up for the lack of outdoor durability of nitrile rubber, and the chemical resistance of nitrile rubber (such as acid and alkali resistance) enhances the corrosion resistance of the overall material, forming a material that is both flexible and durable.

[0028] In some embodiments, the base resin containing isoprene segments or acrylonitrile groups is obtained by mixing 60-120 parts of butyl rubber and 20-60 parts of nitrile rubber. In the above "60-120", the value includes the minimum and maximum values of the range, and each value between the minimum and maximum values. Specific examples include but are not limited to the point values in the embodiment and the following point values: 60, 70, 80, 90, 100, 110, 120; in the above "20-60", the value includes the minimum and maximum values of the range, and each value between the minimum and maximum values. Specific examples include but are not limited to the point values in the embodiment and the following point values: 20, 30, 40, 50, 60.

[0029] In some embodiments, the nitrile rubber is in powder form, and the particle size is preferably 40-80 mesh.

[0030] Powdered nitrile rubber can be directly mixed with other materials during processing without the need for pre-plasticization, greatly simplifying the processing steps and shortening the mixing time. Powdered nitrile rubber is highly dispersible and easy to handle, with fine particles that are easy to disperse evenly during processing, ensuring consistent product quality.

[0031] Furthermore, the solid tackifying resin is at least one of hydrogenated C5 petroleum resin, hydrogenated C9 petroleum resin, rosin resin, hydrogenated rosin resin, water-white rosin resin, rosin pentaerythritol ester, terpene resin, hydrogenated terpene resin, terpene phenol resin and phenolic resin.

[0032] Solid tackifying resin can significantly improve the viscosity of adhesives. Its good compatibility enables it to be mixed with a variety of materials without affecting the performance of other materials. It also has good thermal and chemical stability and can maintain stable performance in high and low temperatures, acid and alkali environments. Therefore, it can maintain good bonding effects in various harsh environments.

[0033] In some embodiments, the solid tackifying resin is preferably a phenolic resin.

[0034] Furthermore, the liquid tackifying resin is polyisobutylene with a molecular weight of 1000-3000.

[0035] As a low-polarity liquid tackifying resin, polyisobutylene can be evenly dispersed inside the colloid during the mixing process. When the temperature changes, its molecular chains migrate to the bonding interface, filling the micropores on the surface of the substrate to form a physical anchoring effect. Polyisobutylene with a molecular weight exceeding 1000 exhibits excellent adhesion, and its adhesion directly increases with the increase of viscosity.

[0036] In some embodiments, the molecular weight of the polyisobutylene is preferably 2000-3000.

[0037] Furthermore, the plasticizer is at least one of white oil and naphthenic oil.

[0038] As plasticizers, white oil and naphthenic oil can significantly improve the physical properties of rubber products, such as strength, wear resistance, and weather resistance, increase their elasticity and toughness, and extend their service life. White oil and naphthenic oil also have good compatibility and lubricity, effectively swelling and diffusing molecules, improving rubber processing properties, and reducing rubber viscosity and increasing its fluidity, making it easier to mix and shape during processing.

[0039] In some embodiments, the plasticizer is preferably white oil.

[0040] In some embodiments, the plasticizer is preferably a naphthenic oil.

[0041] Furthermore, the filler is at least one of kaolin, calcium carbonate, white carbon black and clay.

[0042] Inorganic fillers such as calcium carbonate and kaolin improve the mechanical strength of the mortar through physical filling and surface adsorption effects. After the filler surface is modified with a silane coupling agent, it forms a chemical bond with the rubber matrix, further inhibiting high-temperature thermal expansion.

[0043] In some embodiments, the filler is preferably calcium carbonate.

[0044] Furthermore, the auxiliary agent includes at least one of stearic acid, zinc stearate, an antioxidant and a silane coupling agent.

[0045] Zinc stearate, as a lubricant, can reduce molecular chain breakage during processing. The synergistic effect of the two can extend the weathering life of the putty. Antioxidants block oxidation chain reactions by capturing free radicals. Silane coupling agents, through their unique molecular structure, can chemically react or physically adsorb with inorganic fillers and organic polymers, thereby achieving an effective combination of the two.

[0046] In some embodiments, the auxiliary agent is preferably stearic acid, antioxidant 1010, and silane coupling agent 560.

[0047] To solve the above problems, the present invention further proposes a method for preparing sealing putty, comprising the following steps: S1: Mixing the above-mentioned base resin containing isoprene segments or acrylonitrile groups, polyolefin elastomer, and high-density polyethylene in an internal mixer at a temperature of 110-130° C. for 40-60 minutes to form a base rubber; S2: adding solid tackifying resin, liquid tackifying resin, filler and additives to the base rubber, kneading and mixing at 100-120° C. for 30-50 minutes; feeding the mixed rubber into an extruder, and extruding and molding at 80-100° C. to obtain sealing putty.

[0048] Furthermore, the rotation speed of the internal mixer is 30-50 rpm, and the rotation speed of the kneader is 20-40 rpm.

[0049] In some embodiments, the rotation speed of the internal mixer is 40 rpm, and the rotation speed of the kneader is 30 rpm.

[0050] The following describes the present invention through specific examples and data.

[0051] The information of the raw materials involved in the specific implementation is shown in Table 1: Table 1 Information of raw materials of Examples and Comparative Examples.

[0052]

[0053] Example 1: 60 parts of butyl rubber, 20 parts of nitrile rubber, 20 parts of POE elastomer, 10 parts of HDPE and 160 parts of calcium carbonate were mixed in an internal mixer at a temperature of 120° C. for 40-60 minutes to form a base rubber; Add 10 parts of HDPE, 20 parts of white oil, 20 parts of phenolic resin, 100 parts of polyisobutylene PB2400, 1 part of stearic acid, 1 part of antioxidant 1010 and 5 parts of silane coupling agent KH560 to the base rubber, knead and mix at 100-120°C for 40 minutes; put the mixed rubber into an extruder and extrude it at 80-100°C to obtain sealing putty.

[0054] Example 2: The preparation method is the same as that of Example 1, except that: The parts of the materials are 80 parts of butyl rubber, 60 parts of nitrile rubber, 70 parts of POE, 10 parts of HDPE, 40 parts of white oil, 40 parts of phenolic resin, 120 parts of polyisobutylene PB2400, 220 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0055] Example 3: The preparation method is the same as that of Example 1, except that: The parts of the materials are 100 parts of butyl rubber, 40 parts of nitrile rubber, 60 parts of POE, 20 parts of HDPE, 40 parts of white oil, 40 parts of phenolic resin, 120 parts of polyisobutylene PB2400, 220 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0056] Example 4: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 20 parts of nitrile rubber, 50 parts of POE, 30 parts of HDPE, 40 parts of white oil, 40 parts of phenolic resin, 120 parts of polyisobutylene PB2400, 220 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0057] Example 5: The preparation method is the same as that of Example 1, except that: The parts of the materials are 100 parts of butyl rubber, 40 parts of nitrile rubber, 60 parts of POE, 20 parts of HDPE, 60 parts of white oil, 20 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 190 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0058] Example 6: The preparation method is the same as that of Example 1, except that: The parts of the materials are 100 parts of butyl rubber, 40 parts of nitrile rubber, 60 parts of POE, 20 parts of HDPE, 20 parts of white oil, 60 parts of phenolic resin, 100 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0059] Example 7: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 100 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0060] Example 8: The preparation method is the same as that of Example 1, except that: The parts of the materials are 80 parts of butyl rubber, 20 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 20 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0061] Example 9: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 40 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0062] Comparative Example 1: The preparation method is the same as that of Example 1, except that: The parts of the materials are 30 parts of butyl rubber, 10 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0063] Comparative Example 2: The preparation method is the same as that of Example 1, except that: The parts of the materials are 140 parts of butyl rubber, 80 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0064] Comparative Example 3: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0065] Comparative Example 4: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 10 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0066] Comparative Example 5: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 100 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0067] Comparative Example 6: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of C5 resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0068] Comparative Example 7: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0069] Comparative Example 8: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 5 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0070] Comparative Example 9: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 120 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0071] Comparative Example 10: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0072] Comparative Example 11: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 50 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0073] Comparative Example 12: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 200 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0074] Comparative Example 13: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0075] Comparative Example 14: The preparation method is the same as that of Example 1, except that: The proportions of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 2 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 200 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0076] Comparative Example 15: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 50 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 200 parts of polyisobutylene PB2400, 240 parts of calcium carbonate, 1 part of stearic acid, 1 part of antioxidant 1010, and 5 parts of silane coupling agent KH560.

[0077] Comparative Example 16: The preparation method is the same as that of Example 1, except that: The parts of the materials are 120 parts of butyl rubber, 60 parts of nitrile rubber, 80 parts of POE, 30 parts of HDPE, 60 parts of naphthenic oil, 60 parts of phenolic resin, 150 parts of polyisobutylene PB2400, and 20 parts of calcium carbonate.

[0078] The sealing glue prepared in the above examples and comparative examples was subjected to various performance tests, including room temperature peel strength (25°C), low temperature peel strength (-10°C), high temperature peel strength (60°C), IPX8 waterproof performance test after high and low temperature cycles (-20°C~100°C), and whether the glue flowed completely after high temperature overload at 130°C for 1 hour. The test standards are as follows: (1) Room temperature peel strength (25°C) (on steel plate) test According to GB / T 2792-2014, the sample is tested for peel strength at room temperature. The sample is prepared according to the standard and tested under the conditions to obtain the peel strength.

[0079] (2) Low temperature peel strength (-10℃) (on steel plate) test In accordance with GB / T 2792-2014, a cooling device was used to maintain the test environment at -10°C. The peel strength test was performed on the sample at -10°C. The sample was prepared according to the standard and tested under this condition to obtain the peel strength.

[0080] (3) High temperature peel strength (60°C) (on steel plate) test In accordance with GB / T 2792-2014, a constant temperature heating device was used to maintain the test environment at 60°C. The peel strength test was performed on the sample at 60°C. The sample was prepared according to the standard and tested under this condition to obtain the peel strength.

[0081] (4) IPX8 waterproof performance test after high and low temperature cycle (-20℃~100℃) (for steel plate) Prepare the test sample in accordance with GB / T 4208-2017, place it in a high-low temperature cycler, and then place it in a 1.5m deep water tank for a period of time to observe whether there is water seepage.

[0082] (5) Test whether the mortar flows completely after 130℃ high temperature overload for 1h Prepare the sample according to GB / T 4851-2014, place it in an oven at 130°C for 1 hour, then take it out and observe whether the sealing putty flows.

[0083] The test results are shown in Table 3.

[0084] The components and important preparation variables of Examples 1-9 and Comparative Examples 1-16 are summarized in Table 2.

[0085] Table 2 Components of Examples 1-9 and Comparative Examples 1-16 of the present invention Butyl rubber / part Nitrile rubber / part POE / copy HDPE / part White oil / part Naphthenic oil / part Phenolic resin / part C5 resin / part Polyisobutylene / part Calcium carbonate / portion Stearic acid / part Antioxidant 1010 / portion Silane coupling agent / part Example 1 60 20 20 10 20 / 20 / 100 160 1 1 5 Example 2 80 60 70 10 40 / 40 / 120 220 1 1 5 Example 3 100 40 60 20 40 / 40 / 120 220 1 1 5 Example 4 120 20 50 30 40 / 40 / 120 220 1 1 5 Example 5 100 40 60 20 60 / 20 / 150 190 1 1 5 Example 6 100 40 60 20 20 / 60 / 100 240 1 1 5 Example 7 120 60 80 30 / 60 60 / 150 240 1 1 5 Example 8 80 20 80 30 / 60 20 / 150 240 1 1 5 Example 9 120 60 40 30 / 20 60 / 100 240 1 1 5 Comparative Example 1 30 10 80 30 / 60 60 / 150 240 1 1 5 Comparative Example 2 140 80 80 30 / 60 60 / 150 240 1 1 5 Comparative Example 3 120 60 80 30 / 60 / / 150 240 1 1 5 Comparative Example 4 120 60 80 30 / 60 10 / 150 240 1 1 5 Comparative Example 5 120 60 80 30 / 60 100 / 150 240 1 1 5 Comparative Example 6 120 60 80 30 / 60 / 60 150 240 1 1 5 Comparative Example 7 120 60 / 30 / 60 60 / 150 240 1 1 5 Comparative Example 8 120 60 5 30 / 60 60 / 150 240 1 1 5 Comparative Example 9 120 60 120 30 / 60 60 / 150 240 1 1 5 Comparative Example 10 120 60 80 30 / 60 60 / / 240 1 1 5 Comparative Example 11 120 60 80 30 / 60 60 / 50 240 1 1 5 Comparative Example 12 120 60 80 30 / 60 60 / 200 240 1 1 5 Comparative Example 13 120 60 80 / / 60 60 / 150 240 1 1 5 Comparative Example 14 120 60 80 2 / 60 60 / 150 240 1 1 5 Comparative Example 15 120 60 80 50 / 60 60 / 150 240 1 1 5 Comparative Example 16 120 60 80 30 / 60 60 / 150 20 / / / In accordance with GB / T 2792-2014, GB / T 4208-2017, and GB / T 4851-2014 standards, the sealing adhesives in Examples 1-9 and Comparative Examples 1-16 were subjected to tests for room temperature peel strength (25°C), low temperature peel strength (-10°C), high temperature peel strength (60°C), IPX8 waterproof performance test after high and low temperature cycling (-20°C to 100°C), and complete flow of the adhesive after high temperature overload at 130°C for 1 hour. The test results are recorded in Table 3 below: Table 3. Performance test table of Examples 1-9 and Comparative Examples 1-16 of the present invention

[0086] According to the above test results, it can be seen that the room temperature peel strength of the sealing glue obtained by the various components in Example 1 is 31.2N / 10mm, the low temperature peel strength is 18.1N / 10mm, and the high temperature peel strength is 22.7N / 10mm. The room temperature peel strength of Example 4 is 43.7N / 10mm, the low temperature peel strength is 29.2N / 10mm, and the high temperature peel strength is 29.5N / 10mm. Examples 1, 2, 3, and 4 all passed the IPX8 waterproof performance test (-20℃~100℃) (for steel plate) after high and low temperature cycling and the test of whether the glue flows completely after 130℃ high temperature overload for 1h. In Comparative Example 1, the number of butyl rubber added is 30 parts and the number of butyl rubber added is 10 parts. In Comparative Example 2, the number of butyl rubber added is 140 parts and the number of butyl rubber added is 80 parts. Compared with Example 7, the high temperature peel strength of Comparative Example 1 is 6. 8N / 10mm, and also failed the IPX8 waterproof performance test (-20℃~100℃) (on steel plate) after high and low temperature cycling. After 1h of high temperature overload at 130℃, the glue flowed. The high temperature peel strength of Comparative Example 2 was 13.6N / 10mm, and also failed the IPX8 waterproof performance test (-20℃~100℃) (on steel plate) after high and low temperature cycling. After 1h of high temperature overload at 130℃, the glue flowed. The change in the amount of butyl rubber and nitrile rubber added made the high temperature peel strength of Comparative Examples 1 and 2 very poor. And it can not pass the waterproof and high temperature flow test, in Comparative Example 3, Comparative Example 4 and Comparative Example 5, the added parts of phenolic resin are 0 parts, 10 parts and 100 parts respectively, the high temperature peel strength of Comparative Example 3 is 3.2N / 10mm, and the three also fail the waterproof test in the performance test, Comparative Example 5 fails the high temperature flow test, and in Comparative Example 6, the solid tackifying resin is replaced with ordinary C5 resin, and the high temperature peel strength of Comparative Example 5 is 4.3N / 10mm, and it can not pass the waterproof and high temperature flow test, indicating that the solid tackifying resin and the containing The isoprene segments in the base resin containing isoprene segments or acrylonitrile groups or the acrylonitrile groups in the nitrile rubber undergo condensation reactions to form ether bonds (-O-) or methylene bridges (-CH2-), gradually building a three-dimensional cross-linked network. The cross-linked structure inhibits molecular chain slippage at high temperatures (130°C) and prevents the cement from softening and flowing. In Comparative Examples 7, 8, and 9, the added amounts of POE are 0, 5, and 120 parts, respectively. The low-temperature peel strength of Comparative Example 7 is 3.6 N / 10 mm, and the low-temperature peel strength of Comparative Example 8 is 5.1 N / 10mm, Comparative Examples 7, 8 and 9 all failed the waterproof and high-temperature flow tests. In Comparative Examples 10, 11 and 12, the added amounts of liquid tackifying resin were 0, 5 and 200 parts respectively. Comparative Examples 10 and 11 were unable to complete the low-temperature peel strength test and the high-temperature peel strength test. Compared with Example 7, the amounts of POE and liquid tackifying resin in Comparative Examples 7 to 12 were not within the range of 20-80 parts of the polyolefin elastomer and 100-150 parts of the liquid tackifying resin proposed in the present invention. The gap in low-temperature peel strength, waterproof test and high-temperature flow test shows that POE and liquid tackifying resin improve the low-temperature bonding strength. POE has excellent compatibility with liquid tackifying resin. At low temperatures, the liquid tackifying resin migrates from the inside of the colloid to the interface to form a flexible transition layer, which enhances the wettability to substrates such as metals and plastics, thereby improving the low-temperature bonding strength. In Comparative Examples 13 to 15, the HDPE addition amounts were 0, 2, and 50 parts, respectively, all outside the 10-30 parts HDPE range proposed in the present invention. Comparative Examples 13, 14, and 15 all failed the IPX8 test after high-temperature cycling and the mortar flow test after 130°C high-temperature overload for 1 hour. This demonstrates that when the HDPE addition amount in the formulation is outside the 10-30 parts HDPE range, the resulting sealing mortar exhibits poor high-temperature performance and fails to meet the test standards. In the present invention, the plasticizing effect of the liquid tackifying resin reduces the overall modulus of the mortar, while the cross-linked network of the solid tackifying resin provides rigid support. This ensures the mortar's ability to recover from deformation within high and low temperature ranges (-40°C to 130°C). This ensures that the sealing mortar provided by the present invention not only exhibits good sealing and adhesion properties, but also excellent weather resistance and high and low temperature resistance.

[0087] The above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Those skilled in the art will readily appreciate that the present invention is susceptible to various modifications and variations. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of the present invention.

Claims

1. A sealing putty, characterized in that: The ingredients of the sealing putty are calculated by weight and include: 80-180 parts of base resin containing isoprene segments or acrylonitrile groups, Polyolefin elastomer 20-80 parts, 10-30 parts of high-density polyethylene, 20-60 parts of solid tackifying resin, 100-150 parts of liquid tackifying resin.

2. The sealing putty according to claim 1, wherein The sealing putty further comprises 20-60 parts of a plasticizer, 160-240 parts of a filler and 7-15 parts of an auxiliary agent.

3. The sealing putty according to claim 1, wherein The base resin containing isoprene segments or acrylonitrile groups includes 60-120 parts of butyl rubber and 20-60 parts of nitrile rubber.

4. The sealing putty according to claim 1, wherein The solid tackifying resin is at least one of hydrogenated C5 petroleum resin, hydrogenated C9 petroleum resin, rosin resin, hydrogenated rosin resin, water-white rosin resin, rosin pentaerythritol ester, terpene resin, hydrogenated terpene resin, terpene phenol resin and phenolic resin.

5. The sealing putty according to claim 1, wherein The liquid tackifying resin is polyisobutylene with a molecular weight of 1000-3000.

6. The sealing putty according to claim 2, characterized in that The plasticizer is at least one of white oil and naphthenic oil.

7. The sealing putty according to claim 2, characterized in that The filler is at least one of kaolin, calcium carbonate, white carbon black and clay.

8. The sealing putty according to claim 2, wherein: The auxiliary agent includes at least one of stearic acid, zinc stearate, an antioxidant and a silane coupling agent.

9. A method for preparing the sealing putty according to claim 1, characterized in that: The following steps are involved: Mixing a base resin containing an isoprene segment or an acrylonitrile group, a polyolefin elastomer, and a high-density polyethylene in an internal mixer at a temperature of 110-130° C. for 40-60 minutes to form a base rubber; Adding solid tackifying resin, liquid tackifying resin, filler and additives to the base rubber, kneading and mixing at 100-120° C. for 30-50 minutes; The mixed rubber material is put into an extruder and extruded at 80-100° C. to obtain the sealing putty.

10. The method for preparing the sealing glue according to claim 9, wherein: The speed of the internal mixer is 30-50 rpm, and the speed of the kneader is 20-40 rpm.

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